南大西洋热液沉积物的不同相态提取方法与元素赋存状态

张颖; 杨宝菊; 李传顺; 王小静; 汪虹敏; 刘季花

doi:10.12284/hyxb2021057

南大西洋热液沉积物的不同相态提取方法与元素赋存状态

doi: 10.12284/hyxb2021057

张颖^{1, 2, 3,},
杨宝菊^{1, 2, 3},
李传顺^{1, 2, 3},
王小静^{1, 2, 3},
汪虹敏^{1, 2, 3},
刘季花^{1, 2, 3, ,}

1.
自然资源部第一海洋研究所，山东青岛 266061
2.
自然资源部海洋地质与成矿作用重点实验室，山东青岛 266061
3.
青岛海洋科学与技术试点国家实验室海洋地质过程与环境功能实验室，山东青岛 266237

基金项目: 国家自然科学基金项目（40976038）；国际海域资源调查与开发“十三五”规划项目（DY135-S2-2-03，DY135-S2-2-01）；青岛海洋科学与技术国家实验室海洋地质过程与环境功能实验室开放基金资助项目（MGQNLM-KF201815）；国家重点基础研究发展计划（2013CB429704）

详细信息

作者简介:
张颖（1986-），女，山西省晋中市人，主要从事海洋沉积物元素与同位素分析研究。E-mail：zhangyinghj@163.com

通讯作者:
刘季花（1965-），女，研究员，主要从事海洋沉积地球化学方面研究。E-mail：jihliu@fio.org.cn

中图分类号: P736.4
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出版历程
- 收稿日期: 2020-02-14
- 修回日期: 2020-06-28
- 网络出版日期: 2021-02-25
- 刊出日期: 2021-04-23

Sequential extraction procedure and element occurrence states of hydrothermal sediments from the South Atlantic Ridge

Zhang Ying^{1, 2, 3
,},
Yang Baoju^{1, 2, 3},
Li Chuanshun^{1, 2, 3},
Wang Xiaojing^{1, 2, 3},
Wang Hongmin^{1, 2, 3},
Liu Jihua^{1, 2, 3
, ,}

1.
First Institute of Oceanography, Ministry of Natural Resources, Qingdao 266061, China
2.
Key Laboratory of Marine Geology and Metallogeny, Ministry of Natural Resources, Qingdao 266061, China
3.
Laboratory for Marine Geology and Environment, Pilot National Laboratory for Marine Science and Technology (Qingdao), Qingdao 266237, China

摘要

摘要: 本文对采自南大西洋受不同程度热液活动影响的表层沉积物样品进行了元素和矿物组成分析，并对热液沉积物的碳酸盐相、Fe-Mn氧化物相和残渣态进行了一系列顺序提取实验。选用不同浓度的盐酸羟胺(HH)和醋酸(HAc)混合溶液对样品的Fe-Mn氧化物相进行提取，通过分析不同实验条件下Fe-Mn氧化物相Ti/Nd、Ti/Pb比值和Fe-Mn氧化物相、残渣态的稀土元素(REE)标准化配分模式及Ce和Eu异常值，确定了不同类型热液沉积物样品Fe-Mn氧化物相提取的理想试剂条件均为0.5 mol/L HH和25% HAc混合溶液。研究结果表明，受热液活动影响程度越高，沉积物中Fe、Cu、Zn等元素含量越高，Ca、Sr、Ba含量呈相反趋势，Mn、Pb和REE未受到热液活动明显影响；随着受热液活动影响增强，Ca、Sr、Nd在Fe-Mn氧化物相中所占比例增加，在残渣态中降低，Mn、Co、Ni和Zn呈相反趋势，Cu在碳酸盐相所占比例增加，在残渣态中降低，Pb赋存状态不受热液活动影响，主要赋存于Fe-Mn氧化物相；REE主要赋存于残渣态，沉积物受热液活动影响越明显，残留相对REE富集能力越强，残渣态REE球粒陨石标准化配分模式表现为LREE相对富集越来越不明显的特征。本文研究为进一步了解南大西洋热液沉积物特征和热液活动对沉积物元素赋存状态影响提供了方法和地球化学数据支持。
- 南大西洋 /
- 热液沉积物 /
- 相态提取 /
- 元素赋存状态
Abstract: In this study, elemental and mineral compositions of three surface sediments collected from the South Atlantic Ridge affected by hydrothermal activities of various degrees were analyzed, and series of extraction experiments for carbonate phase, Fe-Mn oxide phase and insoluble residual phase were carried out. Mixed reagent of hydroxylamine hydrochloride (HH) with different concentrations and 25% acetic acid (HAc) were used to extract Fe-Mn oxide phase from the sample. In order to corroborate the reliability of the extracting methods, Ti/Nd and Ti/Pb ratios of the Fe-Mn oxide phase, rare earth elements (REE) patterns as well as δCe and δEu ratios of different chemical phase were used to determine that the ideal reagent conditions for extracting Fe-Mn oxide phase from three different types of hydrothermal sediments were all 0.5 mol/L HH in 25% acetic acid. The results show that the higher the degree of influence of hydrothermal activities, the higher the contents of Fe, Cu, Zn and other elements in the sediments, and the contents of Ca, Sr and Ba show an opposite trend. Manganese, Pb and REE are not significantly affected by hydrothermal activities. As the influence of hydrothermal activity increases, the proportion of Ca, Sr and Nd increases in the Fe-Mn oxide phase and decreases in the residual phase, while Mn, Co, Ni and Zn have an opposite trend, and the proportion of Cu increases in the carbonate phase and decreases in the residual phase. Lead is not affected by the influence strength of hydrothermal activity and mainly occurs in the Fe-Mn oxide phase. REE mainly occur in the residue state. The occurrence state of REE shows that the more significant influence by the hydrothermal activities of the sediments, the more enrichment of REE in the residual phase. And the chondrite-normalized REE patterns of the residual phase exhibit that the enrichment of light REE are less obvious. This study provides methods for extracting hydrothermal fractions and valuable geochemical data for further understanding of the characteristics of hydrothermal sediments and the effects of hydrothermal activities on the occurrence state of elements in the South Atlantic Ridge.
- South Atlantic Ridge /
- hydrothermal sediment /
- sequential leaching /
- element occurrence states

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图 1 南大西洋不同类型热液沉积物样品X射线衍射图

Fig. 1 The XRD patterns of different sediment samples from the South Atlantic

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图 2 不同站位样品元素含量变化

Fig. 2 Changes of element contents of three samples from different areas

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图 3 热液沉积物样品26III-04碳酸盐相中各元素含量随醋酸浓度变化

Fig. 3 Changes of element contents in carbonate phase with the concentration of acetic acid of sample 26III-04

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图 4 样品全岩、碳酸盐相、Fe-Mn氧化物相和残渣态的稀土元素球粒陨石标准化模式图（球粒陨石标准化值据文献[32]）

Fig. 4 Chondrite-normalized REE distribution patterns in bulk sediments of different phases in hydrothermal sediments from South Atlantic (normalization values according to the reference [32])

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图 5 样品中元素赋存状态

Fig. 5 Element occurrence states of different hydrothermal sediments

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表 1 样品全岩及非碳酸盐组分化学分析结果

Tab. 1 The chemical composition of three sediment samples and the carbonate-free fraction

	样品号	Al₂O₃	CaO	Fe₂O₃	K₂O	Na₂O	MgO	MnO	Ti	Al/Ti	Ba	Sr	Co	Ni	Cu	Zn	Cr	V	Mo
全样	33II-12	1.00	48.33	1.94	0.31	1.78	0.75	0.18	446	42.3	162	1620	15	19	69	22	6.35	38	1.62
	26V-04	3.49	41.31	4.17	0.30	2.31	1.91	0.17	2092	31.5	300	1734	23	27	416	112	37	83	1.16
	26III-04	13.33	0.84	25.80	0.21	1.32	15.43	0.21	5071	49.7	9.67	52	110	84	10012	976	163	433	16.12
非碳酸盐	33II-12	11.99	2.35	23.36	1.56	1.00	3.70	1.92	4826	−	1765	143	150	140	791	233	84	612	15.72
	26V-04	13.23	7.66	17.39	0.48	1.84	5.59	0.69	8514	−	1175	181	86	100	1805	314	166	472	4.42
	26III-04	10.33	0.50	25.16	0.21	0.31	13.16	0.21	5340	−	1.98	10	100	83	5259	944	189	581	13.10

	样品号	Pb	Th	U	La	Ce	Pr	Nd	Sm	Eu	Gd	Tb	Dy	Ho	Er	Tm	Yb	Lu	Y
全样	33II-12	11.85	1.15	0.32	11.85	14.10	2.75	11.06	2.43	0.60	2.42	0.41	2.63	0.50	1.38	0.21	1.19	0.18	15.90
	26V-04	23.93	0.90	0.36	10.55	13.63	2.61	11.19	2.62	0.77	2.69	0.48	3.03	0.59	1.74	0.26	1.54	0.24	18.13
	26III-04	12.57	0.55	4.79	5.33	10.68	1.92	9.22	2.90	0.79	3.32	0.67	4.67	0.91	2.81	0.41	2.49	0.42	25.01
非碳酸盐	33II-12	145	10.96	1.31	36.31	169	8.68	34.23	6.99	1.99	7.15	1.23	7.87	1.53	4.41	0.69	4.26	0.66	44.15
	26V-04	107	2.67	0.62	14.64	48.24	4.14	18.03	4.57	1.59	4.96	0.96	6.32	1.27	3.63	0.58	3.54	0.56	32.45
	26III-04	12.91	0.53	4.42	4.56	9.82	1.66	8.16	2.59	0.67	2.84	0.64	4.45	0.91	2.60	0.41	2.55	0.42	23.93
注：氧化物单位为%，其他元素单位为μg/g。

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表 2 不同实验条件下元素回收率（%）

Tab. 2 The recovery rate of elements under different experimental conditions (%)

样品号	C(HH)/（mol·L⁻¹）	Al	Ca	Fe	Mg	Mn	Ti	Sr	Co	Ni	Cu	Zn	Cr	Pb	Nd
26V-04	2	94.7	112.1	92.0	94.7	90.1	95.7	93.7	83.3	122.9	96.7	90.0	122.6	100.8	87.1
	1	93.1	111.9	88.4	93.3	91.4	89.9	93.6	86.1	122.2	96.5	87.2	123.0	97.7	86.2
	0.5	89.4	111.4	88.4	90.5	88.5	88.3	93.5	82.1	119.3	96.1	89.4	112.3	98.3	85.5
	0.25	95.3	112.0	93.2	98.0	92.6	97.1	93.6	87.7	129.3	100.0	91.8	124.6	90.6	88.8
	0.1	91.3	111.4	97.6	88.6	91.1	94.4	93.8	84.1	121.0	111.9	97.9	116.1	121.1	91.2
26III-04	2	102.1	107.0	98.4	100.5	95.8	97.3	98.2	94.6	97.9	92.9	97.9	116.7	92.5	91.5
	1	88.5	98.3	98.2	92.0	95.4	97.6	93.9	92.6	100.0	92.2	97.9	121.1	91.7	92.9
	0.5	95.2	97.4	98.0	95.4	95.7	97.3	93.7	91.5	97.4	93.5	98.4	116.7	91.9	94.4
	0.25	101.8	93.0	97.5	102.2	94.5	97.5	91.7	92.7	99.5	92.8	98.6	123.6	90.0	94.3
	0.1	104.0	92.3	101.5	101.3	96.7	100.5	93.0	92.9	104.9	95.4	102.4	119.6	100.0	94.0

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表 3 不同实验条件下提取出的沉积物各相态百分比（%）

Tab. 3 Proportion of main phases from experimental investigations (%)

C(HH)/(mol·L⁻¹)	样品33II-12			样品26V-04			样品26III-04
C(HH)/(mol·L⁻¹)	碳酸盐相	Fe-Mn氧化物相	残渣态	碳酸盐相	Fe-Mn氧化物相	残渣态	碳酸盐相	Fe-Mn氧化物相	残渣态
2	92.57	1.33	6.10	76.71	3.05	20.24	5.14	10.86	84.00
1	92.54	1.07	6.38	78.10	2.79	19.11	5.54	9.32	85.14
0.5	92.58	0.90	6.52	78.23	2.56	19.20	5.46	7.92	86.62
0.25	92.95	0.69	6.37	77.37	1.99	20.64	5.38	6.59	88.02
0.1	−	−	−	77.11	2.09	20.80	5.23	5.10	89.67
注：−表示无数据。

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表 4 不同实验条件下代表性元素在各相态中百分比(%)

Tab. 4 Percentage of representative elements in different chemical phase from leaching tests (%)

样品号	相态	C(HH)/(mol·L⁻¹)	Al₂O₃	CaO	Fe₂O₃	MgO	MnO	Ti	Sr	Co	Ni	Cu	Zn	Cr	Pb	Nd
33II-12	碳酸盐相		4.67	99.61	2.53	56.06	13.35	0.28	99.07	0.00	56.99	30.41	26.19	4.74	2.02	73.61
	Fe-Mn氧化物相	2	4.21	0.12	30.66	4.91	82.65	2.18	0.30	90.96	23.63	26.01	24.87	11.09	90.69	15.68
		1	3.98	0.13	27.64	4.59	83.68	1.41	0.35	90.07	26.02	24.35	25.67	8.42	84.21	16.47
		0.5	3.13	0.12	22.97	3.89	83.74	0.96	0.32	89.25	23.96	19.98	22.02	7.55	68.25	13.62
		0.25	2.68	0.11	19.84	3.32	82.71	0.47	0.30	88.01	22.90	17.92	19.89	6.38	47.78	11.57
	残渣态	2	90.91	0.21	66.69	36.33	2.65	97.53	0.56	9.04	14.13	41.69	47.69	82.95	7.24	8.72
		1	91.36	0.27	69.83	39.34	2.97	98.31	0.58	9.93	16.99	45.24	48.14	86.84	13.77	9.92
		0.5	92.15	0.24	74.56	38.74	3.41	98.76	0.58	10.75	17.37	50.43	52.43	87.20	29.82	11.93
		0.25	92.43	0.26	77.60	39.37	4.58	99.24	0.56	11.99	18.16	50.76	53.77	88.31	50.24	13.69
26V-04	碳酸盐相		4.49	95.80	2.04	27.45	8.89	0.09	97.38	0.00	30.36	28.80	39.50	6.08	1.51	60.67
	Fe-Mn氧化物相	2	5.75	0.21	39.15	6.72	73.26	2.70	0.83	63.68	21.83	40.33	28.93	9.87	90.86	19.08
		1	5.32	0.21	36.78	5.44	74.10	1.49	0.86	64.37	20.32	39.47	28.25	7.70	84.61	18.83
		0.5	4.58	0.18	32.69	3.67	73.95	0.79	0.81	65.57	18.01	34.29	25.90	6.33	65.32	16.35
		0.25	4.07	0.16	29.85	3.14	72.32	0.36	0.78	61.64	16.48	28.79	24.04	5.12	51.39	14.83
		0.1	3.96	0.18	26.40	3.65	73.18	0.21	0.82	64.03	16.02	20.75	21.71	5.03	23.48	13.02
	残渣态	2	89.76	3.99	58.81	65.83	17.85	97.20	1.79	36.32	47.80	30.87	31.58	84.05	7.64	20.25
		1	90.11	3.81	61.10	66.70	17.13	98.41	1.67	35.63	49.13	31.66	30.98	86.23	13.83	19.87
		0.5	90.67	3.45	65.18	67.60	17.00	99.11	1.68	34.43	50.71	36.71	34.31	87.02	33.13	21.83
		0.25	91.47	3.98	68.13	70.33	19.03	99.55	1.78	38.36	54.67	43.33	37.24	88.89	46.94	25.63
		0.1	91.39	3.40	71.68	67.00	18.02	99.70	1.89	35.97	53.15	54.36	41.95	88.55	75.26	29.04
26III-04	碳酸盐相		0.25	34.76	1.87	1.30	2.49	0.00	58.50	3.56	0.55	56.66	4.39	0.19	0.99	10.29
	Fe-Mn氧化物相	2	3.13	22.60	26.96	3.07	25.97	0.51	23.98	30.41	5.09	30.57	21.60	5.21	86.90	50.91
		1	2.57	16.22	21.73	2.66	24.51	0.22	19.94	29.72	4.15	27.77	15.23	3.59	80.86	47.42
		0.5	1.81	12.92	17.23	2.01	23.71	0.10	18.02	25.61	3.12	25.47	11.28	2.82	68.97	41.70
		0.25	1.25	11.32	14.36	1.53	22.85	0.04	16.46	24.80	2.43	22.72	8.51	2.02	56.00	35.10
		0.1	0.91	10.22	13.57	1.46	22.92	0.02	16.21	24.73	2.43	22.47	7.33	2.04	42.27	31.73
	残渣态	2	96.62	42.64	71.17	95.63	71.53	99.49	17.52	66.03	94.36	12.77	74.01	94.60	12.11	38.80
		1	97.14	45.95	76.39	95.93	72.99	99.77	18.90	66.64	95.32	15.11	80.38	96.22	18.14	42.44
		0.5	97.92	48.90	80.89	96.62	73.80	99.90	20.69	70.71	96.33	18.22	84.35	96.99	30.04	48.32
		0.25	98.49	48.68	83.76	97.20	74.62	99.96	20.90	71.57	97.03	20.54	87.13	97.80	42.98	54.91
		0.1	98.84	49.47	84.61	97.25	74.61	99.98	22.01	71.64	97.05	22.34	88.48	97.78	56.81	58.24

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表 5 不同实验条件下各相态中元素含量和元素比

Tab. 5 Element concentrations and element ratios in different chemical phase from leaching tests

样品号	相态	C(HH)/(mol·L⁻¹)	Al₂O₃	CaO	Fe₂O₃	MgO	MnO	Ti	Sr	Co	Ni	Cu	Zn	Cr	Pb	Nd	Al/Ti	Ti/Pb	Ti/Nd
33II-12	碳酸盐相		0.05	58.15	0.05	0.40	0.02	1.13	1450	0.00	17	22	6	0.39	0.23	7.52	228	4.95	0.15
	Fe-Mn氧化物相	2	3.88	6.27	50.78	3.09	10.99	787	404	835	589	1 589	521	67	921	143	26	0.85	5.48
		1	3.58	6.33	44.97	2.84	11.48	500	440	907	664	1 525	549	61	822	145	38	0.61	3.45
		0.5	3.32	6.95	45.73	2.81	14.25	396	476	1076	709	1 537	577	58	833	142	44	0.48	2.79
		0.25	3.59	8.44	49.69	3.13	18.57	244	589	1393	880	1 698	659	64	740	157	78	0.33	1.56
	残渣态	2	13.79	1.88	18.20	3.78	0.06	5796	125	13.67	58	433	171	83	12	13	12.59	478	440
		1	13.82	2.28	19.10	4.09	0.07	5851	124	16.82	73	476	173	105	23	15	12.50	259	398
		0.5	13.49	1.99	20.45	3.86	0.08	5632	121	17.84	71	534	189	93	50	17	12.68	112	329
		0.25	13.40	2.21	21.02	4.02	0.11	5625	120	20.52	75	520	193	96	84	20	12.61	67	281
26V-04	碳酸盐相		0.19	57.34	0.10	0.64	0.02	2.42	2045	0.00	13	150	51	3.54	0.47	7.65	419	5.15	0.32
	Fe-Mn氧化物相	2	6.23	3.26	49.25	3.99	3.74	1775	444	393	240	5 328	956	146	720	61	19	2.47	29.07
		1	6.19	3.40	48.59	3.47	4.19	1007	500	449	243	5 687	989	125	710	65	33	1.42	15.45
		0.5	5.56	3.14	47.00	2.47	4.41	567	513	474	229	5 350	1010	102	600	61	52	0.94	9.29
		0.25	6.80	3.72	58.34	2.96	5.82	369	640	614	293	6 029	1244	118	561	74	98	0.66	4.97
		0.1	6.02	3.87	51.31	2.95	5.50	197	641	580	253	4 618	1136	102	325	64	162	0.61	3.10
	残渣态	2	14.65	9.12	11.14	5.88	0.14	9613	144	33.71	79	614	157	187	9	9.75	8.07	1056	985
		1	15.30	9.23	11.78	6.22	0.14	9692	142	36.22	86	666	158	203	17	10.04	8.36	572	966
		0.5	14.71	8.28	12.51	6.08	0.14	9535	142	33.22	86	765	179	187	41	10.88	8.17	235	877
		0.25	14.72	8.91	12.81	6.37	0.15	9796	140	36.77	93	873	185	197	49	12.34	7.95	199	794
		0.1	13.99	7.53	14.02	5.45	0.14	9463	148	32.81	84	1 217	221	181	105	14.26	7.83	90	664
26III-04	碳酸盐相		0.66	5.97	9.09	3.84	0.10	2.45	568	70.79	8.67	10 0847	802	6.91	2.20	16.61	1417	1.12	0.15
	Fe-Mn氧化物相	2	3.92	1.87	62.98	4.38	0.49	231	112	291	38.58	26 192	1899	91	93	39.55	90	2.48	5.84
		1	3.25	1.43	59.04	4.04	0.53	118	104	324	37.43	27 490	1560	76	100	43.53	145	1.18	2.72
		0.5	2.89	1.33	55.05	3.74	0.61	63	110	325	32.29	30 133	1368	68	101	45.83	244	0.62	1.37
		0.25	2.57	1.34	54.78	3.65	0.70	29	118	383	30.84	32 031	1242	62	96	46.29	477	0.30	0.62
		0.1	2.48	1.55	69.64	4.48	0.92	19	153	495	42.03	42 069	1433	78	104	53.84	683	0.18	0.36
	残渣态	2	15.65	0.46	21.50	17.65	0.17	5843	10.60	81.72	92.53	1 414	841	214	1.68	3.90	14.18	3485	1499
		1	13.46	0.45	22.72	15.99	0.17	5797	10.79	79.57	94.22	1 638	902	223	2.46	4.27	12.29	2360	1359
		0.5	14.34	0.46	23.61	16.41	0.17	5692	11.58	82.07	91.17	1 970	935	213	4.01	4.85	13.33	1421	1173
		0.25	15.17	0.43	23.94	17.41	0.17	5616	11.27	82.81	92.24	2 169	952	224	5.53	5.42	14.30	1016	1036
		0.1	15.28	0.43	24.71	16.96	0.17	5683	11.81	81.57	95.49	2 380	985	213	7.96	5.62	14.23	714	1010
注：氧化物单位为%，其他元素单位为μg/g。

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表 6 不同实验条件下各相态稀土元素δCe和δEu值

Tab. 6 δCe ratios and δEu ratios of different chemical phase from leaching tests in hydrothermal sediments on the South Atlantic

C(HH)/（mol·L⁻¹）	33II-12				26V-04				26III-04
	Fe-Mn氧化物相		残渣态		Fe-Mn氧化物相		残渣态		Fe-Mn氧化物相		残渣态
	δCe	δEu	δCe	δEu	δCe	δEu	δCe	δEu	δCe	δEu	δCe	δEu
2	2.02	0.68	1.12	1.26	1.75	0.73	1.14	1.13	0.86	1.05	0.87	0.50
1	1.82	0.64	1.22	1.13	1.64	0.68	1.22	1.09	0.86	1.01	0.84	0.51
0.5	2.00	0.66	1.40	1.03	1.60	0.71	1.34	1.26	0.87	0.98	0.87	0.58
0.25	1.98	0.68	1.45	0.88	1.57	0.73	1.28	1.16	0.86	1.02	0.86	0.57
0.1	−	−	−	−	1.55	0.74	1.41	1.10	0.88	1.00	0.81	0.67
注：−表示无数据。

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